CN207659354U - Utilize the device of sulfide in partition board extractive distillation column methanol removal - Google Patents
Utilize the device of sulfide in partition board extractive distillation column methanol removal Download PDFInfo
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- CN207659354U CN207659354U CN201721205307.0U CN201721205307U CN207659354U CN 207659354 U CN207659354 U CN 207659354U CN 201721205307 U CN201721205307 U CN 201721205307U CN 207659354 U CN207659354 U CN 207659354U
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Abstract
The utility model is related to the devices using sulfide in partition board extractive distillation column methanol removal, device includes de- trechmannite tower, partition board extractive distillation column, condenser, reboiler and return tank, extraction and distillation technology is coupled with partition board tower technology, low-temp methanol is washed trechmannite component in recycle methanol and is steamed by de- trechmannite column overhead, controls trechmannite constituent content in tower reactor and is less than 5mg/kg.The device of sulfide in a kind of extractive distillation column methanol removal using partition board provided by the utility model is designed by exchanging heat, makes full use of extractant heat to exchange heat, energy-saving effect is notable.
Description
Technical field
The utility model belongs to technical field of coal chemical industry, relates generally to a kind of using in partition board extractive distillation column methanol removal
The device of sulfide.
Background technology
Develop the New Coal Chemical technology based on coal gasification, realize the clean utilization of coal resources, is to solve China
Pollution that caused by coal burning, oil shortage realize resource, the important research direction of the energy, environment global optimization and sustainable development.Sulfide
It is one of the major pollutants in coal gas, equipment burn into catalyst poisoning and environmental pollution can be caused.Vulcanization species in coal gas
Class and content are related with the area of coal mining and type, generally all contain sulfur dioxide, hydrogen sulfide, carbonyl sulfur, methyl mercaptan, second
The thio-alcohols sulfide such as mercaptan, propanethiol.
It is desulfurization and decarburization technique that current Coal Chemical Engineering Project generally uses that low-temp methanol, which is washed,.Traditional low-temp methanol washing process
Flow includes mainly raw material air cooling, acid gas washing removing (absorbing part), effective gas is recycled in the flash distillation of middle pressure, low pressure flash returns
Receive CO2 gases, nitrogen air lift (H2S enrichments), methanol hot recycling and the several parts of washing tail gas.The technique absorbability is strong, acid
Gas-selectively is excellent, operation is relatively stablized.But the technology there is purified gas total sulfur and contain when handling the unstripped gas of high sulfur content
Measure exceeded problem.To solve the problems, such as this, fresh methanol is needed to frequently replace and supplements, the waste of methanol greatly increases.
It is more and more urgent to the clean utilization demand of sulphur coal (S >=1.0%) with the development of China's coal chemical technology,
The problem of needing for traditional low-temp methanol washing process develops a kind of efficient methanol desulfurization technology, improves cheap
The utilization rate of sulphur coal reduces the waste that low-temp methanol washes recycle methanol, all has for society and enterprise extremely important
Meaning.
Utility model content
The purpose of the utility model is to overcome in place of the deficiencies in the prior art, provide a kind of efficient utilization partition board extraction
Take the device of sulfide in rectifying column methanol removal.
The technical scheme adopted by the utility model is that:
The device of sulfide in a kind of extractive distillation column methanol removal using partition board;Including de- trechmannite tower, partition board extraction essence
Evaporate tower, the main reboiler in bottom of tower, bottom of tower auxiliary reboiler, multiple overhead condensers, feed preheater, extractant cooler, multiple
Tower bottom reboiler, multiple overhead condensers, multiple return tanks;
The de- trechmannite tower top is provided with vapor phase exit and liquid-phase reflux entrance, and middle and upper part is provided with feed(raw material)inlet, bottom
It is provided with second outlet, the return tank top of de- trechmannite tower is provided with condensate inlet and gas phase not condensate extraction mouth, and bottom is set
It is equipped with bypass outlet and liquid phase extraction mouth;De- trechmannite top of tower vapor phase exit is connect with de- trechmannite overhead condenser, and condenser goes out
Mouth is connect with return tank top condensate inlet, and condensate extraction mouth is not connect return tank upper gaseous phase with claus oven pipeline, is returned
Stream pot bottom bypass outlet is connect with tower top liquid phase reflux inlet, and liquid phase extraction mouth is connect with lightweight sulphur storage tank;In de- trechmannite tower
Portion feed(raw material)inlet is connect with de- trechmannite tower feed preheater, and the feed preheater other end connects rectisol system;De- trechmannite
Tower bottom second outlet is divided into two by-pass lines, and one connect with the de- main reboiler in trechmannite bottom of tower, and another auxiliary with de- trechmannite bottom of tower
Reboiler is helped to connect;
The partition board extracting rectifying tower dividing plates are located at the middle and upper part in tower, and divider height accounts for entire king-tower total filler height
30%-70%;Partition board is welded to connect with inner wall of tower, and partition board extractive distillation column is divided into left rectifying section, right rectifying section and public is carried
Evaporate section;
The left rectifying section of partition board extractive distillation column is extractive distillation column, and top is provided with vapour phase extraction mouth and liquid-phase reflux enters
Mouthful, middle and upper part is provided with extractant entrance, and middle part is equipped with feed(raw material)inlet, and the return tank top of partition board extractive distillation column is provided with cold
Lime set entrance, bottom are provided with product extraction mouth and liquid-phase reflux outlet;Vapour phase extraction mouth and overhead condensation at the top of left rectifying section
Device connects, and condensator outlet is connect with return tank top condensate inlet, and return tank bottoms produces the qualified methanol of mouth connection
Storage tank, return tank bottom liquid phases bypass outlet are connect with left rectifying section liquid-phase reflux entrance, and extractant entrance is cooled down with extractant
Device connects, and feed(raw material)inlet takes off the outlet of trechmannite tower bottom of tower with partition board extractive distillation column and connects;
Vapour phase extraction mouth and liquid-phase reflux entrance are provided at the top of the right rectifying section of plate extractive distillation column, plate extractive distillation column
Return tank top is provided with condensate inlet, and bottom is provided with liquid phase extraction mouth and liquid-phase reflux outlet;Vapour phase produces mouth and tower
Condenser connection is pushed up, condensator outlet is connect with return tank top condensate inlet, return tank bottom liquid phases bypass outlet and the right side
Rectifying section liquid-phase reflux entrance connects, and liquid phase extraction mouth is connect with heavy sulphur storage tank;
The partition board extracting rectifying tower bottom is provided with liquid-phase outlet, which is divided into two by-pass lines, one with bottom of tower again
Device connection is boiled, another connect with the main reboiler hot-fluid stock suction line in de- trechmannite tower bottom of tower, and the main reboiler hot-fluid stock in bottom of tower goes out
Mouth pipeline is connect with de- trechmannite tower feed preheater hot-fluid stock suction line, feed preheater hot-fluid stock outlet line and extractant
Cooler hot-fluid stock suction line connects, and extractant cooler hot-fluid stock outlet line extracts with the left rectifying section of partition board extractive distillation column
Agent entrance is taken to connect.
Moreover, the de- trechmannite column overhead produces trechmannite component, controls trechmannite constituent content in tower reactor and be less than 5mg/kg, T1
Tower atmospheric operation, reflux ratio 6-12.
Moreover, the concrete technology control condition of the partition board extractive distillation column T2 is:Left rectifying section overhead extraction methanol production
Product, right rectifying section overhead extraction higher boiling sulfur compound;Partition board extractive distillation column decompression operation, operating pressure-0.04--
0.06Mpa, left rectifying section reflux ratio 1-3,47.5-51.5 DEG C of tower top temperature, right rectifying section reflux ratio 2-5, tower top temperature 48.5-
52.5 DEG C, 174-178 DEG C of column bottom temperature.
Moreover, the extractant in N-Methyl pyrrolidone, N- N-formyl morpholine Ns, sulfolane, tributyl phosphate one
Kind or two or more mixtures.
Moreover, the mixing quality ratio of described two extractants is 1-4, the addition of extractant is 1-5 times of matter of inlet amount
Amount ratio.
Moreover, right rectifying section tower adds second block of lateral steel plate, second block of lateral steel plate is added, rectifying master is welded to
Tower surveys wall, will be shut at the top of right rectifying section, entire right rectifying section is located at the centre of king-tower.
It the advantages of the utility model and has the beneficial effect that:
1, in a kind of extractive distillation column methanol removal using partition board provided by the utility model sulfide device, will will extract
It takes distillation process to be carried out in a rectifying column with extractant regeneration PROCESS COUPLING, reduces equipment investment and energy consumption to greatest extent.
2, in a kind of extractive distillation column methanol removal using partition board provided by the utility model sulfide device, by changing
Thermal design makes full use of extractant heat to exchange heat, and energy-saving effect is notable.
3, sulfur removal technology described in the utility model is compared with conventional distillation sulfur removal technology, and one, small investment, at least save one
The equipment investment of rectifying column, a reboiler and a condenser;Two, product total sulfur content is low and high income, passes through extractant
With the interaction of sulfide, achievees the purpose that deep desulfuration and improve product recovery rate, the left rectifying section tower top methanol of next door tower
Middle total sulfur content is less than 5mg/kg, meets the design requirement that low-temp methanol washes recycle methanol;Three, low energy consumption, by reasonably changing
Thermal design, extractant heat are fully utilized, and energy-saving effect is notable.
Description of the drawings
The technological process of sulfide in Fig. 1 the utility model partition board extractive distillation column methanol removals.
T1 takes off trechmannite tower, and T2 partition board extractive distillation columns, the main reboiler in the bottoms of tower E1, the bottoms of tower E2 assist reboiler, E3 tower tops cold
Condenser, E4 feed preheaters, E5 extractant coolers, E6 tower bottom reboilers, E7-T2 overhead condensers one, E8 overhead condensers
Two, V1 return tank, the left tower return tanks of V2, the right tower return tanks of V3;
The sulfur-rich methanol of 1-, the poor sulphur methanol of 2-, 3- sulfide gas, 4- low boiling point sulfide, 5- regenerating extracting agents, 6- regeneration
Methanol, 7- higher boiling sulfur compounds, 8- partition boards, the left rectifying sections of 9-, the right rectifying sections of 10-, the public stripping sections of 11-.
Specific implementation mode
It is described in further detail below in conjunction with the accompanying drawings and by specific embodiment to the utility model, following embodiment only describes
Property, it is not limited, protection scope of this utility model cannot be limited by this.
Utilize the device of sulfide in partition board extractive distillation column methanol removal;Trechmannite tower, T2 partition boards extraction essence are taken off including T1
Evaporate tower, the main reboiler in the bottoms of tower T1, the bottoms of tower T1 auxiliary reboiler, T1 overhead condensers, T1 feed preheaters, extractant cooler,
The left tower return tank of T2 tower bottom reboilers, T2 overhead condensers one, T2 overhead condensers two, T1 return tanks, T2 and the right towers of T2 return
Flow tank;
The de- trechmannite tower T1, tower top are provided with gaseous phase outlet and liquid-phase reflux entrance, and middle and upper part is provided with raw material and enters
Mouthful, bottom is provided with liquid phase second outlet, and the tops return tank V1 are provided with condensate inlet and gas phase not condensate extraction mouth, bottom
It is provided with bypass outlet and liquid phase extraction mouth;The outlet of T1 top gas phases is connect with T1 overhead condenser E3 entrances, condensator outlet
It being connect with the tops return tank V1 condensate inlet, condensate extraction mouth is not connect return tank V1 upper gaseous phases with claus oven pipeline,
Return tank V1 bottom bypass outlets are connect with T1 tower top liquid phase reflux inlets, and return tank V1 bottom liquid phases produce mouth and stored up with lightweight sulphur
Tank connects;T1 middle feeds entrance is connect with T1 feed preheaters E4, and the E4 other ends connect rectisol system;T1 bottom liquids
Phase second outlet is divided into two by-pass lines, and one connect with the main reboiler E1 in the bottoms of tower T1, and another assists reboiler E2 with the bottoms of tower T1
Connection;
The partition board extractive distillation column T2, partition board are located at the middle and upper part of rectifying king-tower T2, and divider height accounts for entire king-tower
The 30%-70% of total filler height;Partition board is rectangle steel plate, and steel plate is welded to connect with rectifying king-tower T2 inner walls, by rectifying master
T2 points of tower is left rectifying section, right rectifying section and public stripping section;
The left rectifying sections of T2 are extractive distillation column, and top is provided with gas phase extraction mouth and liquid-phase reflux entrance, middle and upper part setting
There are extractant entrance, middle part to be equipped with feed(raw material)inlet, the tops return tank V2 are provided with condensate inlet, and bottom is provided with product extraction
Mouth and liquid-phase reflux outlet;Vapour phase extraction mouth is connect with overhead condenser E7 at the top of left rectifying section, condensator outlet and return tank
Top condensate inlet connection, return tank V1 bottoms produce the qualified methanol tank of mouth connection, and return tank V1 bottom liquid phases are returned
Outflux is connect with left rectifying section liquid-phase reflux entrance, and extractant entrance is connect with extractant cooler E5, feed(raw material)inlet and T1
De- trechmannite tower bottom of tower outlet connection;
It is provided with gas phase extraction mouth at the top of the right rectifying sections of T2 and liquid-phase reflux entrance, the tops return tank V3 are provided with condensate liquid
Entrance, bottom are provided with liquid phase extraction mouth and liquid-phase reflux outlet;Vapour phase extraction mouth is connect with overhead condenser E8, and condenser goes out
Mouth is connect with the tops return tank V3 condensate inlet, return tank V3 bottom liquid phases bypass outlet and right rectifying section liquid-phase reflux entrance
Connection, liquid phase extraction mouth are connect with heavy sulphur storage tank;
The partition board extracting rectifying T2 tower bottoms are provided with liquid phase second outlet, which is divided into two by-pass lines, one
It is connect with tower bottom reboiler E6, another connect with the main reboiler E1 hot-fluids stock suction line in the de- bottoms of tower trechmannite tower T1, E1 hot-fluids
Stock outlet line is connect with T1 feed preheater E4 hot-fluid stock suction lines, E4 hot-fluid stock outlet lines and extractant cooler E5
Hot-fluid stock suction line connects, and E5 hot-fluid stock outlet lines are connect with the left rectifying section extractant entrances of T2.
The invention also discloses the methods using sulfide in partition board extractive distillation column methanol removal simultaneously, including such as
Lower step:Come from low-temp methanol and wash main absorbing tower bottom, total sulfur content is 100-30000mg/kg (predominantly carbonyl sulfur, sulphur
Change hydrogen, sulfur dioxide, methyl mercaptan, ethyl mercaptan, n-propyl mercaptan, n-butyl mercaptan, isoamyl mercaptan, n-amyl mercaptan, dimethyl disulfide,
Methylethyl disulfide, diethyl disulphide) sulfur-rich methanol feedstock, entered by de- trechmannite tower feed(raw material)inlet, trechmannite therein
Component is steamed by de- trechmannite column overhead, and return tank V1 is entered after overhead condenser condenses, not solidifying sulfide (predominantly carbonyl
Sulphur, hydrogen sulfide and sulfur dioxide) it is directly entered claus oven calcining recycling sulphur, a liquid phase component part passes back into tower, a part
Trechmannite component is plucked out of into trechmannite storage tank, is periodically focused on.The sulfur-rich methanol of T1 tower reactors is by the left essence of T2 partition board extractive distillation columns
It evaporates a section feed(raw material)inlet to enter in T2 towers, extractant is entered by left rectifying section middle and upper part extractant entrance, and extracting rectifying process is on a left side
Rectifying section carries out, and under extractant effect, the relative volatility of higher boiling sulfur compound and methanol increases, and qualified methanol is by this section of tower
Top steams, and right rectifying section overhead vapor phase higher boiling sulfur compound enters return tank V2, Partial Liquid Phase vulcanization after being condensed by condenser E8
Object produces, and another part liquid phase sulfide enters right rectifying section reflux.It is first and de- light that next door tower tower reactor regenerates complete extractant
The main reboiler E1 in sulphur tower bottom of tower heat exchange, after-heat by feed preheater E4 to raw material preheating, then through extractant cooler E5
It is cooled to 49 DEG C and enters the recycling of next door tower.
Wherein, T1 column overheads produce trechmannite component, control trechmannite constituent content in tower reactor and are less than 5mg/kg, T1 tower normal pressures behaviour
Make, reflux ratio 6-12.
The concrete technology control condition of partition board extractive distillation column T2 is:Left rectifying section overhead extraction methanol product, right rectifying
Section overhead extraction higher boiling sulfur compound;T2 tower decompression operations, operating pressure-0.04-- 0.06Mpa, left rectifying section reflux ratio 1-
3,47.5-51.5 DEG C of tower top temperature, right rectifying section reflux ratio 2-5,48.5-52.5 DEG C of tower top temperature, column bottom temperature 174-178
℃。
One kind in N-Methyl pyrrolidone, N- N-formyl morpholine Ns, sulfolane, tributyl phosphate of the extractant or
Two or more mixtures.
When variety classes extractant mixes, the mixing quality ratio of two kinds of extractants is 1-4, and the addition of extractant is charging
1-5 times (mass ratio) of amount.
Right rectifying section tower can add second block of lateral steel plate, be welded to rectifying king-tower and survey wall, by right rectifying section top
Portion is shut, and entire right rectifying section is located at the centre of king-tower.
Embodiment 1
A method of using sulfide in partition board extractive distillation column methanol removal, detailed process is as follows:
Sulfur-rich methanol comes from the prewashing section that low-temp methanol is washed, and is characterized as methanol 95.40553% (wt%), carbonyl sulfur
0.00216%, hydrogen sulfide 0.043%, methyl mercaptan 0.00405%, ethyl mercaptan 0.0136%, n-propyl mercaptan 0.00872%, positive fourth
Mercaptan 0.00396%, sulfur dioxide 0.01381%, ammonium sulfide 0.00233%, n-amyl mercaptan 0.00253%, dimethyl disulfide
Ether 0.00031%, water 4.5%, rectifying tower packing be screen waviness structured packing, 20 pieces of T1 desulfurizing towers theoretical plate, atmospheric operation,
Reflux ratio 8,40 pieces of T2 partition board extractive distillation columns theoretical plate, decompression operation, operating pressure -0.05MPa, left rectifying section reflux ratio
1.5, right rectifying section reflux ratio 3.Prewashing methanol inlet amount is 50kg/h, and extractant feed amount is that 100kg/h enters partition board extraction
Rectifying column, after device is stablized, 38.4 DEG C of T1 tower top temperatures, 67.1 DEG C of T1 column bottom temperatures, 47.6 DEG C of the left rectifying section tower top temperatures of T2,
49.5 DEG C of the right rectifying section tower top temperatures of T2,176.9 DEG C of T2 column bottom temperatures.Equipment continuous operation 12h takes the left rectifying section of T2 tower tops again
Raw methanol product carries out content and total sulfur content measures.
After testing, the total sulfur content in embodiment in the left rectifying section methanol product of T2 tower tops, methanol content are as shown in the table:
Embodiment | Total sulfur (mg/kg) | Methanol purity (%) |
Embodiment 1 | 2.9 | 99.91 |
Claims (4)
1. the device of sulfide in a kind of extractive distillation column methanol removal using partition board;It is characterized in that:Including de- trechmannite tower, every
Plate extractive distillation column, the main reboiler in bottom of tower, bottom of tower auxiliary reboiler, multiple overhead condensers, feed preheater, extractant cooling
Device, multiple tower bottom reboilers, multiple overhead condensers, multiple return tanks;
The de- trechmannite tower top is provided with vapor phase exit and liquid-phase reflux entrance, and middle and upper part is provided with feed(raw material)inlet, bottom setting
There is second outlet, the return tank top of de- trechmannite tower is provided with condensate inlet and gas phase not condensate extraction mouth, and bottom is provided with
Bypass outlet and liquid phase produce mouth;De- trechmannite top of tower vapor phase exit is connect with de- trechmannite overhead condenser, condensator outlet and
The condensate inlet connection of return tank top, condensate extraction mouth is not connect return tank upper gaseous phase with claus oven pipeline, return tank
Bottom bypass outlet is connect with tower top liquid phase reflux inlet, and liquid phase extraction mouth is connect with lightweight sulphur storage tank;It is former in the middle part of de- trechmannite tower
Material entrance is connect with de- trechmannite tower feed preheater, and the feed preheater other end connects rectisol system;De- trechmannite bottom of tower
Portion's second outlet is divided into two by-pass lines, and one connect with the de- main reboiler in trechmannite bottom of tower, and another assists again with de- trechmannite bottom of tower
Boil device connection;
The partition board extracting rectifying tower dividing plates are located at the middle and upper part in tower, and divider height accounts for entire king-tower total filler height
30%-70%;Partition board is welded to connect with inner wall of tower, and partition board extractive distillation column is divided into left rectifying section, right rectifying section and public is carried
Evaporate section;
The left rectifying section of partition board extractive distillation column is extractive distillation column, and top is provided with vapour phase extraction mouth and liquid-phase reflux entrance, in
Top is provided with extractant entrance, and middle part is equipped with feed(raw material)inlet, and the return tank top of partition board extractive distillation column is provided with condensate liquid
Entrance, bottom are provided with product extraction mouth and liquid-phase reflux outlet;Vapour phase extraction mouth connects with overhead condenser at the top of left rectifying section
It connecing, condensator outlet is connect with return tank top condensate inlet, and return tank bottoms produces the qualified methanol tank of mouth connection,
Return tank bottom liquid phases bypass outlet is connect with left rectifying section liquid-phase reflux entrance, and extractant entrance connects with extractant cooler
It connects, feed(raw material)inlet takes off the outlet of trechmannite tower bottom of tower with partition board extractive distillation column and connects;
Vapour phase extraction mouth and liquid-phase reflux entrance, the reflux of plate extractive distillation column are provided at the top of the right rectifying section of plate extractive distillation column
Tank top is provided with condensate inlet, and bottom is provided with liquid phase extraction mouth and liquid-phase reflux outlet;Vapour phase produces mouth and tower top is cold
Condenser connects, and condensator outlet is connect with return tank top condensate inlet, return tank bottom liquid phases bypass outlet and right rectifying
Section liquid-phase reflux entrance connection, liquid phase extraction mouth are connect with heavy sulphur storage tank;
The partition board extracting rectifying tower bottom is provided with liquid-phase outlet, which is divided into two by-pass lines, one and tower bottom reboiler
Connection, another connect with the main reboiler hot-fluid stock suction line in de- trechmannite tower bottom of tower, the main reboiler hot-fluid stock outlet in bottom of tower
Line is connect with de- trechmannite tower feed preheater hot-fluid stock suction line, and feed preheater hot-fluid stock outlet line is cooled down with extractant
Device hot-fluid stock suction line connects, extractant cooler hot-fluid stock outlet line and the left rectifying section extractant of partition board extractive distillation column
Entrance connects.
2. the device of sulfide in the extractive distillation column methanol removal according to claim 1 using partition board;It is characterized in that:
The de- trechmannite column overhead produces trechmannite component, controls trechmannite constituent content in tower reactor and is less than 5mg/kg, takes off trechmannite tower normal pressure behaviour
Make, reflux ratio 6-12.
3. the device of sulfide in the extractive distillation column methanol removal according to claim 1 using partition board;It is characterized in that:
The concrete technology control condition of the partition board extractive distillation column is:Left rectifying section overhead extraction methanol product, right rectifying section tower top
Produce higher boiling sulfur compound;Partition board extractive distillation column decompression operation, operating pressure-0.04-- 0.06Mpa, left rectifying section reflux
Than 1-3,47.5-51.5 DEG C of tower top temperature, right rectifying section reflux ratio 2-5,48.5-52.5 DEG C of tower top temperature, column bottom temperature 174-
178℃。
4. the device of sulfide in the extractive distillation column methanol removal according to claim 1 using partition board;It is characterized in that:
The right rectifying section tower adds second block of lateral steel plate, is welded to rectifying king-tower and surveys wall, will be shut at the top of right rectifying section, whole
A right rectifying section is located at the centre of king-tower.
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Address after: 210023 No. 6 Jiaolan Road, Qixia District, Nanjing, Jiangsu Province Co-patentee after: Ningxia Baofeng energy group Limited by Share Ltd Patentee after: China Construction Installation Group Co., Ltd. Address before: 210023 No. 6 Wenlan Road, Qixia District, Nanjing, Jiangsu Province Co-patentee before: Ningxia Baofeng energy group Limited by Share Ltd Patentee before: China Construction Industrial Equipment Installation Co., Ltd. |
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